1/9/2018 » Titration of Citric Acid CHEM 103 Lab

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Titration of Citric Acid

September 4, 2016

by S. Choi, R. Gleason, and K. Jewett (with edits by R. Sandwick and M. J. Simpson)

Learning goals: maintain safety in a chemistry laboratory, work collaboratively with a lab partner, follow
instructions to complete a laboratory experiment, collect and analyze experimental data, explain likely sources
of experimental error

Introduction

Citric acid is a polyprotic acid (can release three H+s) that is a bit on the weak side (i.e., tends not to ionize
completely). In solution in fruit juices, it lets a small portion of the H+ go, however this small amount of acid is
enough to create a pH = ~3 solution and a sharp taste on the palate. If strong base is added to citric acid it will
sequentially lose its three protons in the following manner:

Citric acid deprotonation in 3 steps. Credit:

CrystEngComm, 2014,16, 3387-3394

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Background

In today’s experiment we are going to determine the amount of citric acid in a fruit juice by using a base-acid
reaction. If we know exactly how much base we add to completely remove all the H+ ions (called
“deprotonating”) from the citric acid in the juice, we can calculate how much citric acid is in the solution. This
process of employing one reagent of known concentration to determine a compound of unknown concentration
in solution is termed titration. It usually involves slowly adding small amounts of the titrant to the analyte until
a reaction is just barely complete. The apparatus typically used is a buret. The equivalence point (or end point) is
the exact point where all the analyte in solution has reacted. Since the equivalence point of many titrations do
not result in observable changes, end point indicators are added to (are you ready for this?) indicate the end
point.

In this experiment you will use a solution of NaOH to titrate the acid in a fruit juice. To be accurate, the exact
concentration of the NaOH solution you prepare must be known. Powdered NaOH (from which you will make
your solution) is known to slowly decompose upon reaction with CO2 in the air to generate NaHCO3. Thus you
will need to standardize, or precisely determine the concentration, the NaOH solution using a stable primary
standard. Only after you have satisfactorily determined the exact concentration of your NaOH solution can you
accurately determine the citric acid concentration in the fruit juice.

There are several good primary standards for standardizing base solutions, but one of the best and cheapest is the
compound oxalic acid dihydrate, H2C2O4 ● 2 H2O. (Oxalic acid is a natural acid found in rhubarb leaves; it is
toxic so don’t eat it.) It is important to note that the chemical equation (shown below) shows a stoichiometry of
one moles of oxalic acid to every two mole of NaOH in this reaction.

H2C2O4(aq) + 2 NaOH(aq) → C2O42-(aq) + 2 Na+(aq) + 2 H2O(l)

The indicator we will use in both is phenolphthalein, a common indicator of acid-base titration. Phenolphthalein
was the active ingredient in Ex-lax until recently when it was phased out due to its carcinogenicity.

Procedure

Note: do this lab with a partner.

Standardization of a Solution of Sodium Hydroxide

1. Thoroughly clean and rinse with distilled water your supplies: a burette, a 25-mL graduated cylinder, a
500 mL boiling flask, and three 250 or 300-mL Erlenmeyer flasks.
2. Put your NaOH pellets (mass calculated in the pre-lab) in the 500 mL boiling flask. Cover them with a
small amount of water and swirl until they dissolve. The heat of solution produced by the NaOH helps to
speed the dissolving process. Once the pellets are dissolved, fill the flask to the base of the neck. Using
Parafilm, mix the solution thoroughly by inverting several times (the flask not you!). It is best to keep the
flask covered with Parafilm when not in use as CO2 from the air can slowly neutralize the NaOH.
3. Using an analytical balance, weigh out the oxalic acid dihydrate on weighing paper (mass calculated in the
pre-lab). Place it in a clean, clearly labeled Erlenmeyer flask. Note: It is not necessary to weigh out exactly
the amount calculated (although you should be close), however it is imperative that the mass of each
sample of oxalic acid dihydrate be known precisely for each flask. Label each clearly.
4. Dissolve the oxalic acid dihydrate in 25 mL of distilled water and add two drops of phenolphthalein
indicator solution.
5. Repeat steps 3 and 4 for 2 more samples of oxalic acid dihydrate so you have a total of 3 flasks containing
oxalic acid solutions.
6. Rinse your buret once with water and then twice with 5-mL portions of the solution of sodium hydroxide
which you have prepared, draining the solution off through the burette tip into a beaker for waste reagents.
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Fill the buret nearly to the top of the graduated portion with the solution of sodium hydroxide you have
prepared, making sure that the buret tip is completely filled with the solution. Touch the inner wall of a
beaker for waste reagents to the buret tip to remove any hanging drop of solution.
7. Make a preliminary titration using one of your solutions of oxalic acid to learn approximately how the
neutralization proceeds. Place a sheet of white paper under the Erlenmeyer flask so that the color of the
solution is more easily observed. Read and record the position on the burette of the lowest point of the
meniscus of the solution of sodium hydroxide to the nearest one-fifth of a division. Swirl the sample in the
flask, and add sodium hydroxide rather rapidly from the burette until the color of the solution where the
sodium hydroxide is entering the solution begins to linger, then add the base dropwise until, finally, one
drop of the alkaline solution of base changes the colorless solution to a permanent pink, not red. A drop
should not be left hanging on the buret tip. The tip and the walls of the flask should be rinsed with water
from a wash bottle to ensure mixing of all the base with the acid. You probably will overrun the endpoint
in this first titration, but it will provide a useful rough measure of the volume of the sodium hydroxide
solution needed to neutralize the acid and provide you with valuable experience. Read and record the level
of the meniscus in the buret, and compute the volume of basic solution used in the titration.
8. Now titrate the remaining two samples of standard acid, being certain each time to refill the burette nearly
to the top graduation with your sodium hydroxide solution and to record the burette reading. In these runs,
add the sodium hydroxide from the buret very rapidly, again with swirling, until you are ~ 2 mL short of
the volume that you estimate will be needed on the basis of your first titration. Then carefully add base
drop by drop so that you can determine the equivalence point accurately. Record the data for your
titrations in a table and perform the calculations necessary to yield the exact molarity of the NaOH
solution. Show your results to your instructor. The concentrations of your titrations should agree within 1
% of each other.
9. The solution of sodium hydroxide that you have just standardized will be used in Part II, so do not waste
it.

Total acidity of a citrus fruit

Several different types of samples will be available for you to use. When using fruit, squeeze the juice into a
250-mL beaker by cutting the end from the fruit and applying pressure. Use a Büchner funnel and filtering flask
to vacuum filter the juice to remove the pulp. If you are using one of the juice samples, simply use the juice as
is. Deliver 5.00 mL of juice (or 2.00 mL if its highly acidic) into each of two previously weighed (to the nearest
0.001 g) 250-mL flasks. Re-weigh the flasks and its contents to the nearest 0.001g and then dilute the juice to
approximately 50 mL with distilled water. Add two drops of phenolphthalein indicator.

Titrate the prepared juice solution to the phenolphthalein endpoint. Record the final burette reading to the
nearest 0.02 mL. Repeat the experiment until you are satisfied with the precision of successive runs. Put all data
into an appropriate table.

Neutralize waste

Working with your TA, neutralize the excess NaOH solution. Test the pH with pH paper before pouring it down
the drain. Pour titrated solutions down the drain.

Calculations

Calculate the moles of oxalic acid reacted, the moles of NaOH titrated, and the molarity of the NaOH.

Having discovered the exact molarity of the NaOH you used, calculate the number of moles of citric acid in each
sample. Convert this to grams and then to grams citric acid per grams sample. Convert this to a percent citric
acid by weight.

The reaction of sodium hydroxide with citric acid is:

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3 NaOH + H3C6H5O7 → 3 Na+ + 3 H2O + C6H5O73-

Report

Fill out the worksheet for the report. Attach calculations separately. Look up values for citric acid concentration
in juices and compare your value vs. those literature values. Give a proper citation for the source. Optional
survey.

Entry Filed under: Experiments. Posted in Experiments Tags: bureting.

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